EP0560395A1 - Composition détergente non-ionique pulvérulente - Google Patents

Composition détergente non-ionique pulvérulente Download PDF

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EP0560395A1
EP0560395A1 EP93104093A EP93104093A EP0560395A1 EP 0560395 A1 EP0560395 A1 EP 0560395A1 EP 93104093 A EP93104093 A EP 93104093A EP 93104093 A EP93104093 A EP 93104093A EP 0560395 A1 EP0560395 A1 EP 0560395A1
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Prior art keywords
weight
detergent composition
composition
nonionic
total weight
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EP93104093A
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German (de)
English (en)
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EP0560395B1 (fr
Inventor
Mutsumi Kuroda
Yuichi Sakamoto
Yoshinori Otani
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Kao Corp
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Kao Corp
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/1273—Crystalline layered silicates of type NaMeSixO2x+1YH2O
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

  • U. S. Patent No. 4136051 discloses a detergent composition having an improved fluidity and comprising a premixture composed of a crystalline or amorphous aluminosilicate having an ion exchange capacity of 50 mg CaO/g (89 mg CaCO3/g) or more (4% or less of a highly dispersive silica may be used as an oil-absorbent carrier), a nonionic surfactant and optionally an inorganic peroxide capable of forming hydrogen peroxide in water and, incorporated into the premixture, a spray-dried detergent.
  • WO 90/00189 discloses a granular detergent composition produced by homogeneously mixing a porous silicate derivative such as zeolite, bentonite and layer silicate with a water-soluble or water-dispersive nonionic surfactant in such a proportion that the porous silicate derivative content is 30% by weight or more.
  • the layer silicate described in WO 90/00189 has a low ion exchange capacity.
  • the granular detergent composition has the problem of retaining solubility after storage for a long period of time and is unsatisfactory in the detergency as well.
  • This nonionic powdery detergent composition composition can also contain an amorphous alkali metal silicate in an amount of 5% by weight or less based on the total weight of the composition and an alkali metal carbonate in an amount of 15% by weight or less based on the total weight of the composition.
  • the present invention also provides a nonionic powdery detergent composition
  • a nonionic powdery detergent composition comprising 12 to 50% by weight, based on the total weight of the composition, of (a) a nonionic surfactant having a melting point of 40°C or below, 3 to 60% by weight, based on the total weight of the composition, of (b) a crystalline layer silicate represented by the formula (I), 5 to 30% by weight, based on the total weight of the composition, of (c) a porous oil-absorbent carrier having an oil absorbability of 80 ml/100 g or more and 1 to 5% by weight, based on the total weight of the composition, of (d) a polyethylene glycol having a weight average molecular weight of 4000 to 20000: M2Si x O (2x+1) ⁇ y(H2O) (I) wherein M represents an alkali metal atom and x and y are respectively 1.5 ⁇ x ⁇ 4 and y ⁇ 25, that is 0 ⁇
  • This nonionic powdery detergent composition can also contain an amorphous alkali metal silicate in an amount of 5% by weight or less based on the total weight of the composition and an alkali metal carbonate in an amount of 15% by weight or less based on the total weight of the composition.
  • the nonionic powdery detergent composition further contains, preferably, an optional component and the process further comprises, preferably, mixing the homogeneous mixture with a detergent assistant or an additive as an optional component.
  • the nonionic surfactant (a) to be used in the present invention is a liquid or a slurry at 40°C. Namely, the nonionic surfactant (a) has a melting point of 40°C or below and, therefore, is excellent in soil removal, foaming and foam breaking.
  • a polyoxyethylene alkyl ether comprising a straight-chain or branched, primary or secondary alcohol having 10 to 20 carbon atoms, preferably 10 to 15 carbon atoms and particularly preferably 12 to 14 carbon atoms and ethylene oxide added thereto in such a manner that the average number of moles of addition thereof is 5 to 15, preferably 6 to 12 and still preferably 6 to 10, is preferably used as a main nonionic surfactant.
  • the polyoxyethylene alkyl ether contains a large amount of an adduct of an alkyl ether with ethylene oxide wherein the number of moles of addition of ethylene oxide is small. It is preferred to use a polyoxyethylene alkyl ether wherein the content of an adduct having the number of moles of addition of ethylene oxide of 0 to 3 is 35% by weight or less, preferably 25% by weight or less.
  • the nonionic powdery detergent composition according to the present invention contains the nonionic surfactant (a) in an amount of 12 to 50% by weight, preferably 12 to 35% by weight, and still preferably 15 to 30% by weight based on the total weight of the composition.
  • 0.1 g of a sample is weighed and dispersed in 100 ml of an aqueous solution of 500 ppm, as CaCO3, of CaCl2. After the dispersion is stirred at 25°C for 10 minutes, it is rapidly filtered (through a 0.2- ⁇ m filter). 50 ml of deionized water is added to 10 ml of the filtrate.
  • the nonionic powdery detergent composition according to the present invention contains the crystalline layer silicate (b) in an amount of 3 to 60% by weight, preferably 5 to 40% by weight, and particularly preferably 20 to 40% by weight based on the total weight of the composition.
  • U.S. Patent No. 4664839 describes a process for producing the crystalline layer silicate (b), and the crystalline layer silicate (b) is generally produced by baking an amorphous vitreous sodium silicate at 200 to 1000°C to render the sodium silicate crystalline.
  • the synthetic process is described in detail in, for example, Phys. Chem. Glasses., 7 . 127-138 (1966) and Z. Kristallogr., 129 , 396-404 (1969).
  • the crystalline layer silicate (b) is available in particulate, powdery and granular forms, for example, from Hoechst under the trade name of "Na-SKS-6" ( ⁇ -Na2Si2O5).
  • the porous oil-absorbent carrier (c) in the present invention is a carrier having an oil absorbability of 80 ml/100 g or more, preferably 150 ml/100 g or more, still preferably 200 ml/100 g or more and most preferably 200 to 800 ml/100 g.
  • the oil absorbability is a value measured according to JIS K 6220.
  • the porous oil-absorbent carrier (c) is particularly preferably a silica derivative containing silicon in an amount, calculated as SiO2, of 30% by weight or more and preferably 40% by weight or more, as determined with no hydrate present. Namely, the content of silicon in the porous oil-absorbent carrier (c) is represented by a value calculated as SiO2.
  • Examples of such a porous oil-absorbent carrier include Tokusil AL-1 (manufactured by Tokuyama Soda Co., Ltd.), Nipsil NA (manufactured by Nippon Silica Industrial Co., Ltd.), Carplex #100 (manufactured by Shionogi Pharmaceutical Co., Ltd.) and Sipernat D10 (manufactured by DEGUSSA).
  • Examples of the oil-absorbent amorphous aluminosilicate include an oil-absorbent carrier commercially available under the trademark of Tixolex 25 (manufactured by Kofran Chemical Co., Ltd.).
  • a clayey substance such as smectites which is one of the natural minerals, has a two dimentional structure, and thus causes the deterioration in the solubility of the detergent composition when it is incorporated into the detergent composition. Therefore, use of such a clayey substance in the present invention is unfavorable.
  • oil-absorbent carriers have scarcely any cation exchange capacity.
  • An oil-absorbent carrier having a cation exchange capacity is advantageous because it serves also as a builder for the detergent.
  • the oil-absorbent carrier having a high oil absorbability and a high cation exchange capacity include oil-absorbent amorphous aluminosilicates represented by the formula (1): a(M2O) ⁇ Al2O3 ⁇ b(SiO2) ⁇ c(H2O) (1) wherein M represents an alkali metal atom and a, b and c each represent the number of moles of the respective component, wherein generally 0.7 ⁇ a ⁇ 2.0, 0.8 ⁇ b ⁇ 4 and c represents an arbitrary positive number.
  • Oil-absorbent amorphous aluminosilicates represented by the formula (2) are particularly preferred: Na2O ⁇ Al2O3 ⁇ b(SiO2) ⁇ c(H2O) (2) wherein b is 1.8 to 3.2 and c is 1 to 6.
  • the above-descried amorphous aluminosilicate having a high oil absorbability and a high ion exchange capacity which may be used in the present invention may be produced as follows.
  • An alkalescent aqueous solution of an alkali metal aluminate having a molar ratio of M2O (wherein M represents an alkali metal atom) to Al2O3 of 1.0 to 2.0 and a molar ratio of H2O to M2O of 6.0 to 500 is added at a temperature of 15 to 60°C, preferably 30 to 50°C, under vigorous stirring to an aqueous solution of an alkali metal silicate having a molar ratio of SiO2 to M2O of 1.0 to 4.0 and a molar ratio of H2O to M2O of 12 to 200.
  • the aqueous solution of an alkali metal silicate may be added to the alkalescent aqueous solution of an alkali metal aluminate. Then, the formed white precipitate slurry is heat-treated at a temperature of 70 to 100°C, preferably 90 to 100°C for 10 minutes to 10 hours, preferably 10 minutes to 5 hours, and then filtered. The precipitate on the filter was washed and dried to provide a product.
  • an amorphous aluminosilicate oil-absorbent carrier having an ion exchange capacity of 100 CaCO3 mg/g or more and an oil absorbability of 200 ml/100 g or more and preferably 200 to 800 ml/100 g, can be easily produced.
  • the pH value of the dispersion containing 5% by weight of the porous oil-absorbent carrier is measured according to JIS K 6220. Namely, about 5 g of a sample is weighed into a hard conical flask, and 100 ml of water free from carbonic acid (carbon dioxide) is added thereto. The conical flask is stoppered and then is shaken for 5 min. After shaking, a pH value of the resultant dispersion is measured according to the glass electrode method (see 7.2.3 of JIS Z 8802).
  • a nonionic powdery detergent composition which does not exhibit any deterioration in its solubility even when stored under high-humidity conditions can be produced through the selection of an oil-absorbent carrier having a pH value of the 5% by weight dispersion thereof of 9.0 or greater.
  • the oil-absorbent carrier is one wherein the amount of dissolution of the oil-absorbent carrier is 0.5 g or less as measured according to the method which comprises dispersing 10 g of the oil-absorbent carrier in 100 ml of a 2% aqueous NaOH solution, stirring the dispersion at a constant temperature of 25°C for 16 hours and determining the SiO2 content of the filtrate by colorimetry (Regarding the colorimetry, reference may be made to "Yukagaku", vol. 25, p.
  • Oil-absorbent carriers of this type as well fall within the scope of the present invention.
  • Perlite 4159 manufactured by Dicalite Orient Co., Ltd.
  • an oil-absorbent carrier capable of satisfying more strict requirements that the pH value of the 5% by weight dispersion thereof is 9.0 or greater and that the amount of dissolution thereof in 100ml of a 2% aqueous NaOH solution is 0.5 g or less.
  • oil-absorbent carrier which can satisfies the above-described requirements include "Na-Mordenite HSZ-640 NAA" manufactured by Tosoh Corporation and can be found also in amorphous aluminosilicates represented by the above formula (2).
  • the nonionic powdery detergent composition according to the present invention may contain (d) a polyethylene glycol having a weight average molecular weight of 4000 to 20000 in an amount of 1 to 5% by weight, preferably 1 to 3% by weight.
  • a polyethylene glycol having a weight average molecular weight of 4000 to 20000 in an amount of 1 to 5% by weight, preferably 1 to 3% by weight.
  • a carbonate particularly an alkali metal carbonate such as sodium carbonate
  • an alkali metal carbonate such as sodium carbonate
  • the sodium carbonate include heavy sodium carbonate (heavy ash) and light sodium carbonate (light ash), and the average particle diameter thereof is 10 to 2000 ⁇ m, preferably 100 to 1000 ⁇ m.
  • a synthetic crystalline aluminosilicate (e) into the composition of the present invention.
  • the amount of incorporation thereof is preferably less than 10% by weight based on the total weight of the composition.
  • the nonionic powdery detergent composition of the present invention will have the following composition.
  • nonionic powdery detergent composition comprising 15 to 45% by weight, based on the total weight of the composition, of (a) a nonionic surfactant having a melting point of 40°C or below, 5 to 30% by weight, based on the total weight of the composition, of (b) a crystalline layer silicate represented by the formula (I), 10 to 30% by weight, based on the total weight of the composition, of (c') an amorphous aluminosilicate having an oil absorbability of 100 ml/100 g or more and represented by the formula (3) and 10 to 30% by weight, based on the total weight of the composition, of (e) a synthetic crystalline aluminosilicate, with the proviso that the total content of the nonionic surfactant (a), the crystalline layer silicate (b), the amorphous aluminosilicate (c') and the synthetic crystalline aluminosilicate (e) is 75% by weight or more based on the total weight of the
  • the amorphous aluminosilicate (c') is preferably prepared by allowing at least one acid agent selected from the group consisting of an inorganic acid, an organic acid and an acid salt to exist in a reaction system during a reaction of an alkali metal aluminate with an alkali metal silicate in the production of the amorphous aluminosilicate and allowing the reaction to proceed with the pH value of the reaction system being adjusted to 8 to 14.
  • the synthetic crystalline aluminosilicate (e) is one generally called zeolite and represented by the formula (10): l(M2O) ⁇ Al2O3 ⁇ m(SiO2) ⁇ n(H2O) (10) wherein M represents an alkali metal atom, l, m and n each represent the number of moles of the respective component, wherein generally 0.7 ⁇ l ⁇ 1.5, 0.8 ⁇ m ⁇ 6 and n represents an arbitrary positive number.
  • a synthetic crystalline aluminosilicate represented by the formula (11) is preferred: Na2O ⁇ Al2O3 ⁇ m'(SiO2) ⁇ n'(H2O) (11) wherein m' is 1.8 to 3.0 and n' is a number of 1 to 6.
  • Preferred examples of the crystalline aluminosilicate (e) include synthetic zeolites having an average primary particle diameter of 0.1 to 10 ⁇ m including types A and X zeolites.
  • the zeolite is incorporated in the form of a powder and/or particles which are prepared by drying and aggregating a zeolite slurry.
  • the amorphous alkali metal silicate which can be present in the detergent composition according to the present invention is one having a SiO2/M2O (wherein M represents an alkali metal atom, e.g., sodium and/or potassium) ratio of from 0.5 to 4.0, and is generally incorporated into the detergent composition as an water soluble alkaline salt or used as a corrosion inhibitor for a metal.
  • M represents an alkali metal atom, e.g., sodium and/or potassium
  • the content of the amorphous alkali metal silicate is less than 5% by weight, preferably 1% by weight or less based on the total weight of the composition. When the content of the amorphous alkali metal silicate is 5% by weight or more, the solubility of the detergent composition tends to be remarkably lower.
  • the alkali metal carbonate which can be present in the detergent composition according to the present invention may be a carbonate of sodium or potassium or a mixture of the sodium salt with the potassium salt. Among them, sodium carbonate is preferred in the present invention. Sodium carbonate is as described above.
  • the powdery detergent composition of the present invention usually contains an optional component such as a detergent assistant, an additive and the like which is usually used in detergent compositions.
  • the additive include inorganic electrolytes such as sodium sulfate, inorganic chelating agents such as sodium tripolyphosphate, organic chelating agents such as an aminopolyacetate and a polyacrylate, anti-redeposition agents such as carboxymethylcellulose, enzymes such as protease, lipase, cellulase and amylase, antioxidants, fluorescent dyes, blueing agents and perfumes.
  • the nonionic powdery detergent composition of the present invention has a bulk density of about 0.6 to 1.2 g/ml, preferably 0.7 to 0.9 g/ml.
  • the nonionic powdery detergent composition according to the present invention may be prepared by gradually adding or spraying the nonionic surfactant (a) onto a mixture of powdery components comprising the crystalline layer silicate (b) and the porous oil-absorbent carrier (c) under stirring to prepare a homogeneous mixture and, if necessary, mixing the homogeneous mixture with one or more of the optional components.
  • the nonionic powdery detergent composition according to the present invention may also be prepared by gradually adding or spraying the nonionic surfactant (a) onto a mixture of powdery components comprising the crystalline layer silicate (b) and the porous oil-absorbent carrier (c) under stirring to prepare a homogeneous mixture, adding the polyethylene glycol (d) in a molten state to the homogeneous mixture to prepare a base for the nonionic powdery detergent composition and, if necessary, mixing the base with one or more of optional components.
  • the mixture of powdery components comprises the crystalline layer silicate (b), the porous oil-absorbent carrier (c) and the carbonate.
  • the nonionic powdery detergent composition of the present invention can be easily produced by gradually adding or spraying a liquid nonionic surfactant while mixing powdery components including the crystalline layer silicate, the porous oil-absorbent carrier and optionally the carbonate, etc., to prepare a homogeneous mixture and mixing the homogeneous mixture with minor components such as a perfume and an enzyme, a surface modifier and a bleaching agent when the composition is used as a bleaching detergent composition.
  • the particle diameter of the powdery detergent composition is large (200 to 1000 ⁇ m, preferably 300 to 700 ⁇ m), a further improvement in the properties of the detergent powder during storage for a long period of time can be attained.
  • a batch kneader (Bench Kneader PNV-1 available from Irie Shokai Co., Ltd.) was charged with 3% by weight of a beef tallow soap, an oil-absorbent carrier (c) having properties given in Tables 1 and 2 and a crystalline layer sodium silicate (b) [Na-SKS-6 (manufactured by Hoechst); particle diameter : 50 to 150 ⁇ m; cation exchange capacity : 280 mg CaCO3/g] in respective amounts specified in Tables 3 and 4, a balancing amount of sodium carbonate (average particle diameter : 200 ⁇ m), 3% by weight of sodium polyacrylate (average molecular weight : 7000) and 0.5% by weight of a fluorescent dye.
  • a liquid nonionic surfactant (a) in an amount specified in Tables 3 or 4 was gradually fed into the kneader and then 2% by weight of a melt of a polyethylene glycol (d) having a weight average molecular weight of 12000 was added thereto to provide a base for a powdery detergent composition having an average particle diameter of 385 ⁇ m. Further, 0.5% by weight of an enzyme, 0.3% by weight of a perfume and 3% by weight of zeolite 4A were added to the base and mixed with the base to provide a final detergent product having the above-described composition (which were partially given in Tables 3 or 4).
  • the detergent product was subjected to a test on bleeding, a test on the solubility after a lapse of time and a test on the detergency against a fatty acid soil.
  • a box provided with no top sheathing and having a size of 10.2 cm in length ⁇ 6.2 cm in width ⁇ 4 cm in height was made of a coated carton (640 g/m2), and four corners of the box was stapled. 100 g of a sample was placed in this box, and an acrylic resin plate (15 g) and a lead plate (250 g) (total weight: 265 g) were put on the sample. Then, the box was allowed to stand in a thermohygrostat at 30°C and 80 %RH for 7 days. The degree of bleeding on the coated carton after the test was judged based on the following criteria:
  • a powdery detergent product was placed in a Petri dish and allowed to stand at 30°C and 50 %RH for 3 days. 0.83 g of the powder was then sampled and added into 1 l of tap water at 10°C. The mixture was stirred by means of a magnetic stirrer for 10 min and filtered through a 200-mesh wire gauze, and solid matter remaining on the wire gauze was dried to determine the percentage filtration residue (%).
  • Washing was conducted by means of a Terg-O-Tometer, 100 rpm) under the following conditions: bath ratio: 1/60 water temp.: 35°C washing time: 15 min with calcium-hardened water rinsing: 5 min with calcium-hardened water (use is made of running water) hardness of water: 8° DH (calcium-hardened water) concentration of detergent product: 0.1% by weight.
  • the obtained powder was found to comprise 29.6% by weight of Al2O3, 52.4% by weight of SiO2 and 18.0% by weight of Na2O (1.0Na2O ⁇ Al2O3 ⁇ 3.01SiO2).
  • the Ca ion scavenging capacity and oil absorbability thereof were 165 mg CaCO3/g and 265 ml/100 g, respectively.
  • a 5% dispersion of the powder had a pH value of 10.2, and the solubility of the powder in 100 ml of a 2 wt.% aqueous NaOH solution was 0.10 g.
  • a 1000-ml reaction vessel equipped with a baffle was charged with 55 g of a 6% by weight aqueous sodium carbonate solution prepared in Synthesis Example 1, 51.04 g of an aqueous sodium aluminate solution having a water content of 50% by weight and 25 g of ethanol, and a reaction was allowed to proceed at 40°C over a period of 20 minutes under vigorous stirring while dropwise adding 268.5 g of an aqueous JIS No. 3 sodium silicate solution which was prepared by diluting JIS No. 3 sodium silicate with water twice as much as the sodium silicate and 0.5 g of calcium chloride dihydrate. The pH value was adjusted to 11 with citric acid throughout the reaction. After the completion of the reaction, the system was aged at 40°C for 30 minutes.
  • the obtained powder was found to comprise 29.3% by weight of Al2O3, 52.2% by weight of SiO2, 17.7% by weight of Na2O and 0.8% by weight of CaO (0.99Na2O ⁇ 0.05CaO ⁇ Al2O3 ⁇ 3.03SiO2).
  • the Ca ion scavenging capacity and oil absorbability thereof were 164 mg CaCO3/g and 310 ml/100 g, respectively.
  • a 5% dispersion of the powder had a pH value of 10.3, and the solubility of the powder in 100 ml of a 2 wt.% aqueous NaOH solution was 0.07 g.
  • An agitation tumbling granulator (a Lödige mixer) was charged with 3% by weight of a sodium salt of a beef tallow fatty acid, a crystalline layer sodium silicate (b) [Na-SKS-6 (manufactured by Hoechst); particle diameter: 50 to 150 ⁇ m; cation exchange capacity: 280 mg CaCO3/g], the amorphous aluminosilicate (c') produced in Synthesis Examples 1 or 2, a zeolite (e) and a salt in respective amounts specified in Table 5 and 0.5% by weight of a fluorescent dye.
  • a liquid nonionic surfactant (a) [a synthetic alcohol (C12 ⁇ 14) ethoxylate having a melting point of 15°C, an average number of moles of added ethylene oxide of 7 and a number of carbon atoms of alcohol of 12 to 14] in an amount specified in Table 5 was gradually introduced into the mixer, and then 2% by weight of a melt of a polyethylene glycol (d) having a weight average molecular weight of 8000 and further 0.5% by weight of an enzyme (0.3% by weight of protease and 0.2% by weight of cellulase), 0.5% by weight of a perfume and 2% by weight of water were added thereto and mixed with each other to provide a detergent product having the composition given in Table 5.
  • a synthetic alcohol (C12 ⁇ 14) ethoxylate having a melting point of 15°C, an average number of moles of added ethylene oxide of 7 and a number of carbon atoms of alcohol of 12 to 14 was gradually introduced into the mixer, and then 2% by weight of a melt of a

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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EP93104093A 1992-03-12 1993-03-12 Composition détergente non-ionique pulvérulente Expired - Lifetime EP0560395B1 (fr)

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JP5316892 1992-03-12
JP53168/92 1992-03-12

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EP0560395A1 true EP0560395A1 (fr) 1993-09-15
EP0560395B1 EP0560395B1 (fr) 1997-08-13

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US (1) US5654265A (fr)
EP (1) EP0560395B1 (fr)
AU (1) AU3518193A (fr)
DE (1) DE69312987T2 (fr)
ES (1) ES2104980T3 (fr)
TW (1) TW240243B (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5496486A (en) * 1994-06-30 1996-03-05 Amway Corporation Process for increasing liquid surfactant loading in free flowing powder detergents
EP0816485A1 (fr) * 1996-07-04 1998-01-07 The Procter & Gamble Company Procédé de préparation de compositions détergentes
US6069124A (en) * 1997-05-30 2000-05-30 Lever Brothers Company Division Of Conopco, Inc. Granular detergent compositions and their production
US6174852B1 (en) 1996-01-22 2001-01-16 Kao Corporation High-density powdered detergent composition
US6191095B1 (en) 1997-05-30 2001-02-20 Lever Brothers Company, A Division Of Conopco, Inc. Detergent compositions
US6221831B1 (en) 1997-05-30 2001-04-24 Lever Brothers Company, Division Of Conopco, Inc. Free flowing detergent composition containing high levels of surfactant
US6303558B1 (en) 1997-05-30 2001-10-16 Lever Brothers Co., Division Of Conopco Detergent composition containing at least two granular components
US6936577B2 (en) 2001-10-19 2005-08-30 Unilever Home Products And Care Usa, Division Of Conopco, Inc. Detergent compositions
EP0781320B2 (fr) † 1994-09-13 2013-10-16 Kao Corporation Procede de lavage

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JP3810854B2 (ja) 1996-01-22 2006-08-16 花王株式会社 高密度粉末洗剤組成物
US5863887A (en) * 1997-12-01 1999-01-26 Precision Fabrics Group, Inc. Laundry compositions having antistatic and fabric softening properties, and laundry detergent sheets containing the same
US6130193A (en) * 1998-02-06 2000-10-10 Precision Fabrics Group, Inc. Laundry detergent compositions containing silica for laundry detergent sheets
DE19943254A1 (de) 1999-09-10 2001-03-15 Clariant Gmbh Bleichaktive Metallkomplexe
DE19960744A1 (de) * 1999-12-16 2001-07-05 Clariant Gmbh Granulares Alkalischichtsilicat-Compound
GB0111862D0 (en) * 2001-05-15 2001-07-04 Unilever Plc Granular composition
GB0111863D0 (en) * 2001-05-15 2001-07-04 Unilever Plc Granular composition
JP2008521995A (ja) * 2004-11-30 2008-06-26 エルジー ハウスホールド アンド ヘルス ケア エルティーディー． 衣類の肌触りを向上させることができる粉末洗剤組成物及びその製造方法
KR101392380B1 (ko) * 2007-02-21 2014-05-07 주식회사 엘지생활건강 산성형태의 수용성 고분자를 함유하는 분말세제 입자 및그의 제조방법
EP3181675B2 (fr) 2015-12-17 2022-12-07 The Procter & Gamble Company Composition de détergent de lave-vaisselle automatique
EP3181671A1 (fr) 2015-12-17 2017-06-21 The Procter and Gamble Company Composition de detergent de lave-vaisselle automatique
EP3181676B1 (fr) 2015-12-17 2019-03-13 The Procter and Gamble Company Composition de detergent de lave-vaisselle automatique

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US5635467A (en) * 1994-06-30 1997-06-03 Amway Corporation Powdered composition exhibiting increased liquid surfactant loading for free flowing powder detergents
EP0781320B2 (fr) † 1994-09-13 2013-10-16 Kao Corporation Procede de lavage
US6174852B1 (en) 1996-01-22 2001-01-16 Kao Corporation High-density powdered detergent composition
EP0816485A1 (fr) * 1996-07-04 1998-01-07 The Procter & Gamble Company Procédé de préparation de compositions détergentes
US6069124A (en) * 1997-05-30 2000-05-30 Lever Brothers Company Division Of Conopco, Inc. Granular detergent compositions and their production
US6191095B1 (en) 1997-05-30 2001-02-20 Lever Brothers Company, A Division Of Conopco, Inc. Detergent compositions
US6221831B1 (en) 1997-05-30 2001-04-24 Lever Brothers Company, Division Of Conopco, Inc. Free flowing detergent composition containing high levels of surfactant
US6303558B1 (en) 1997-05-30 2001-10-16 Lever Brothers Co., Division Of Conopco Detergent composition containing at least two granular components
US6936577B2 (en) 2001-10-19 2005-08-30 Unilever Home Products And Care Usa, Division Of Conopco, Inc. Detergent compositions

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DE69312987D1 (de) 1997-09-18
EP0560395B1 (fr) 1997-08-13
TW240243B (fr) 1995-02-11
AU3518193A (en) 1993-09-16
US5654265A (en) 1997-08-05
DE69312987T2 (de) 1998-01-15
ES2104980T3 (es) 1997-10-16

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